AU597690B2 - Carbon electrodes - Google Patents
Carbon electrodes Download PDFInfo
- Publication number
- AU597690B2 AU597690B2 AU75671/87A AU7567187A AU597690B2 AU 597690 B2 AU597690 B2 AU 597690B2 AU 75671/87 A AU75671/87 A AU 75671/87A AU 7567187 A AU7567187 A AU 7567187A AU 597690 B2 AU597690 B2 AU 597690B2
- Authority
- AU
- Australia
- Prior art keywords
- transition metal
- electrode
- carbon
- binder
- present
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Ceased
Links
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title description 4
- 229910052723 transition metal Inorganic materials 0.000 claims description 44
- 150000003624 transition metals Chemical class 0.000 claims description 42
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 23
- 229910052799 carbon Inorganic materials 0.000 claims description 21
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 14
- 239000002245 particle Substances 0.000 claims description 14
- 239000002243 precursor Substances 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 9
- 239000011230 binding agent Substances 0.000 claims description 8
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 7
- 239000011737 fluorine Substances 0.000 claims description 7
- 229910052731 fluorine Inorganic materials 0.000 claims description 7
- 229910052759 nickel Inorganic materials 0.000 claims description 7
- 229910052720 vanadium Inorganic materials 0.000 claims description 7
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 7
- 239000006185 dispersion Substances 0.000 claims description 6
- 239000003575 carbonaceous material Substances 0.000 claims description 5
- 229910017052 cobalt Inorganic materials 0.000 claims description 5
- 239000010941 cobalt Substances 0.000 claims description 5
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 5
- 239000003792 electrolyte Substances 0.000 claims description 5
- 239000007791 liquid phase Substances 0.000 claims description 4
- 239000013110 organic ligand Substances 0.000 claims description 4
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 claims description 4
- 239000011233 carbonaceous binding agent Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical class C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 claims description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 235000003270 potassium fluoride Nutrition 0.000 claims description 2
- 239000011698 potassium fluoride Substances 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- BWLBGMIXKSTLSX-UHFFFAOYSA-N 2-hydroxyisobutyric acid Chemical compound CC(C)(O)C(O)=O BWLBGMIXKSTLSX-UHFFFAOYSA-N 0.000 claims 1
- 102100038824 Peroxisome proliferator-activated receptor delta Human genes 0.000 claims 1
- -1 acetyl- Chemical class 0.000 claims 1
- 239000000446 fuel Substances 0.000 claims 1
- 108091008765 peroxisome proliferator-activated receptors β/δ Proteins 0.000 claims 1
- 230000007704 transition Effects 0.000 claims 1
- 239000010408 film Substances 0.000 description 4
- 230000027756 respiratory electron transport chain Effects 0.000 description 3
- 229910001428 transition metal ion Inorganic materials 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 239000002019 doping agent Substances 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000011269 tar Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000011280 coal tar Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 239000003758 nuclear fuel Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000002006 petroleum coke Substances 0.000 description 1
- 239000003209 petroleum derivative Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/24—Halogens or compounds thereof
- C25B1/245—Fluorine; Compounds thereof
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/042—Electrodes formed of a single material
- C25B11/043—Carbon, e.g. diamond or graphene
Description
i_~ji)( b~ go COMMONWEALTH OF AUSTRALIA PATENTS ACT 1952 Form COMPLETE SPECIFICATION FOR OFFICE USE Short Title: Int. C1: T r
I
Application Number: Lodged: Complete Specification-Lodged: Accepted: Lapsed: Published: Priority: This document contains the amendments made under Section 49 and is correct for printing.
Related Art: i TO BE COMPLETED BY APPLICANT S (4 Name of Applicant: Address of Applicant: Actual Inventor: Address for Service: BRITISH NUCLEAR FUELS Plc.
Warrington, Cheshire WA3 6AS, ENGLAND Oliver Raymond Brown and Martyn John Wilmott ii GRIFFITH HASSEL FRAZER 71 YORK STREET SYDNEY NSW 2000
AUSTRALIA
Complete Specification for the invention entitled: CARBON ELECTRODES The following statement is a full description of this invention, including the best method of performing it known to me/us:- 9686A:rk p b
I
;1; t i 41 ttl I i 1114 (494 44 *9 0 o 9 9 U I I I Carbon Electrodes This invention relates to carbon electrodes such as are used in the production of fluorine by electrolysis of a mixed molten salt electrolyte using a porous carbon anode, the electrolyte usually comprising potassium fluoride and hydrogen fluoride.
According to one aspect of the present invention there is provided a carbon electrode for use in the electrolytic production of fluorine, the electrode having at least one transition metal dispersed therein, a major part of the transition metal being present as centres with diameters no greater than 1 x 10 9 metres.
In practice, the transition metal(s) may be dispersed through the entire carbon electrode although it is within the ambit of the invention for the transition metals to be confined to those parts of the electrode which, in use, are or will become (as a result of electrode material loss in the course of electrolysis) exposed to the electrolyte.
According to a second aspect of the invention, in a method of making a carbon electrode in which the electrode is formed by consolidating a mass of carbon particles with a carbonaceous binder and heat-treating the consolidated mass, the carbonaceous material constituting the binder and/or the precursor of the carbon particles is doped with one or more transition metals by ispersing the transition metal as a thermally decomposable organic complex or
A
I L- frui^- ir complexes of the transition metal(s) in said carbonaceous material while the latter is in a liquid phase, whereby subsequent heat treatment decomposes the complexes to provide a fine dispersion of transition metal within the particles and/or the carbon residue of the binder with a major part of the transition metal(s) being present as centres with diameters no greater than 1 x 10 9 metres The transition metal(s) may be dispersed within the particles by incorporating the transition metal within a 10 precursor material which is subsequently carbonised and finely divided to produce the carbon particles and, in this event, it is preferred to combine the transition metal with the precursor while the latter is in a liquid phase so that dispersion of the transition metal on an atomic scale is 15 facilitated. For example, the transition metal may be t i provided in the form of a thermally decomposable organic complex of the metal, eg. the transition metal combined with an organic ligand such as acetyl acetonate, and may be dissolved in a suitable liquid vehicle, such as furfuryl 20 alcohol, for mixing with the liquid phase precursor. The precursor may then be carbonised, the organic ligand being one which will decompose at temperatures within the range normally used in the carbonisation of precursor materials for carbon electrode production. After carbonisation, the precursor may be pulverised to produce particles of conventional size for carbon electrode production and the particles can then be combined with a suitable binder, such
~LJ
t.s i
I
as pitch tar, consolidated and heat treated to produce a porous carbon electrode comprising the particles and the residue of the pitch tar.
The precursor may be a derivative of petroleum or coal-tar, eg. it may be a petroleum derivative from which petroleum coke is conventionally produced for use in 4 r 49 r 0IIr If4 a 4 04 0 e6 o 0 446 a Q O 0 0 0 4 1 o 4 4 o Il :r I *wu- -iLI_.
Ir I 3 carbon electrode manufacture.
The transition metal elements are preferably selected from nickel, vanadium and cobalt and may be used in combination, eg. both nickel and vanadium doping of the precursor and/or binder may be employed.
Although, at present, it is considered desirable to disperse the transition metal on an atomic scale, a coarser dispersion is within the scope of the invention and preferably the dispersion is such that an arbitrary slice of the electrode or electrode part having a thickness of the order of 10-9 metres is sufficiently thick to wholly encompass at least one transition metal f t t site. In practice, it is recognised that some agglomeration of the transition metal atoms/particles may occur during preparation of the precursor for example but preferably a substantial part of the transition metal is dispersed to the extent just mentioned. Expressed in a alternative terms, it is preferred that the major part of the transition metal dopant is present as centres with 20 diameters no greater than 1 x 10- 9 metres.
The or each transition metal is typically present in an amount less than 1.0 atom and preferably up to about 0.1 atom Especially where the transition metal(s) is/are selected from nickel, vanadium and cobalt, the invention has particular application to carbon anodes as used in fluorine-producing electrolytic cells. It is known that 4 operation of fluorine cells leads to the formation at the anode surface of an extremely thin film of carbon monofluoride (CF)x typically of the order of 10 9 metres thick which significantly increases the anode operating voltage needed for efficient cell operation.
The introduction of a very fine dispersion of these transition metals ensures that transition metal ion sites (resulting from oxidation of the transition metal centres present in the fluoride film) are available within the thickness of the (CF)X film thereby facilitating electron transfer between the electrolyte and the anode.
In operation, the anode tends to erode and consequently the (CF)x film is continually following erosion of the anode surface and therefore encompasses fresh transition metal ion sites. The possibility of enhancement of electron transfer by the transition metal ion sites is thought to counteract the effect of the (CF)x film formation which is believed to reduce the probability of electron transfer from HF2 species. Thus the 20 presence of the transition metal dopants, nickel,cobalt and/or vanadium, serves to reduce the anode overvoltage.
Various other aspects and features of the invention will be apparent from the appended claims.
11 4 09 O *d o 0* o *ar 4010'
I
30613
Claims (18)
1. A carbon electrode for use in the electrolytic production of fluorine, wherein at least one transition metal is dispersed therein, a major part of the transition metal being present as centres with diameters n. greater than 1 x 10 9 metres.
2. An electrode as claimed in Claim 1, wherein the or each transition metal is present in an amount less than atom%. 10
3. An electrode as claimed in Claim 2, wherein the or each transition metal is present in an amount up to a-bhet 0.1 atom%.
4. An electrode as claimed in any one of the pirceding Claims, wherein the transition metal(s) is/are selected from nickel, vanadium, and cobalt.
5. An electrode as claimed in any one of the preceding Claims, wherein the electrode comprises a consolidated mass of carbon particles and the residue of a carbonaceous binder, the transition metal(s) being dispersed in the consolidated mass and/or the binder residue.
6. An electrode as claimed in any one of the preceding Claims, wherein the transition metal(s) is/are derived from a thermally decomposed organic complex or complexes of the transition metal(s) incorporated in the carbon particles and/or binder.
7. An electrode as claimed in Claim 6, wherein the S organic complex comprises the transition metal combined L I .1 ;1 o b 0 44 0 0 0 4 0O 4 4 0*4 0 04 r. *P e with an organic ligand in the form of an acetyl- *acetonate.
8. A method of making a carbon electrode in which the electrode is formed by consolidating a mass of carbon particles with a carbonaceous binder and heat-treating the consolidated mass, wherein the carbonaceous material constituting the binder and/or the precursor of the carbon particles is doped with one or more transition metals by dispersing the transition metal as a thermally decomposable organic complex or complexes of the transition meta in said carbonaceous material while the latter is in a liquid phase, whereby subsequent heat treatment decomposes the complexes to provide a fine dispersion of transition metal within the particles and/or 15 the carbon residue of the binder with a major part uf the transition metal(s) being present as centres with diameters no greater than 1 x 10 9 metres.
9. A method as claimed in Claim 8 including combining an organic complex(es) of the transition metal(s) with the 20 liquid carbonaceous material in the presence of a liquid in which the organic complex(es) of the transition metal(s) is/are soluble. A met.hod as rlaimed in Claim i q, wherein (he organi' complex comprises the transi t.i on metal combined w.i th an organic ligand in the form of an acetyl-acetonate.
S
11. A method as claimed in any one of Cleims 8 to wherein the or each transition metal is selected from -u J::i 00 000 4 *4 o 0 e> o o OA~ 00 04 O 0 .9 4 0 00 6 4 0 0.4 0 nr o o o 0 00 4 0 b 060 0 44 nickel, vanadium and cobalt.
12. A method as claimed in Claim 11, wherein nickel and vanadium are both present.
13. A method as claimed in any one of Claims 8-12 wherein the resulting electrode is of a porous structure.
14. A method as claimed in any one of Claims 8 to 13, wherein the quantity of the or each transition metal is selected to provide less than 1.0 atom in the heat treated consolidated mass. 10
15. A method as claimed in Claim 14, wherein said quantity of the or each transition metal provides up to b 0.1 atom in the heat treated consolidated mass.
16. A carbon electrode produced by the method of any one of Claims 8 to 15
17. A process for the electrolytic production of fluorine, wherein there is used as anode(s), one or more electrodes as claimed in any one of Claims 1 to 7 and 16.
18. An electrolytic cell for the production of fluorine comprising, as electrolyte, a mixed molten salt system of 20 potassium fluoride and hydrogen fluoride and, as anode(s), at least one carbon electrode as claimed in any one of Claims 1-7 and 16. DIatcd this 20th day of February, 1990 BRITISH NUCI .AR FUELS PLC By their Pal ~t Attorneys GRIFFITH HACK CO. ~,r i- i il-LI
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
GB8618909A GB2193225B (en) | 1986-08-01 | 1986-08-01 | Carbon electrodes |
GB8618909 | 1986-08-01 |
Publications (2)
Publication Number | Publication Date |
---|---|
AU7567187A AU7567187A (en) | 1988-02-18 |
AU597690B2 true AU597690B2 (en) | 1990-06-07 |
Family
ID=10602130
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
AU75671/87A Ceased AU597690B2 (en) | 1986-08-01 | 1987-07-15 | Carbon electrodes |
Country Status (8)
Country | Link |
---|---|
US (1) | US4915809A (en) |
EP (1) | EP0255225B1 (en) |
JP (1) | JPS6338593A (en) |
AU (1) | AU597690B2 (en) |
CA (1) | CA1315240C (en) |
DE (1) | DE3766564D1 (en) |
GB (1) | GB2193225B (en) |
ZA (1) | ZA875309B (en) |
Families Citing this family (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2729254B2 (en) * | 1988-08-05 | 1998-03-18 | 信淳 渡辺 | Low polarizable carbon electrode |
JPH0784669B2 (en) * | 1988-11-11 | 1995-09-13 | 三井造船株式会社 | Carbonaceous electrode |
JPH03232988A (en) * | 1990-02-06 | 1991-10-16 | Toyo Tanso Kk | Carbon electrode, method and device for electrolyzing hf-containing molten salt using the same |
CA2071235C (en) * | 1991-07-26 | 2004-10-19 | Gerald L. Bauer | Anodic electrode for electrochemical fluorine cell |
JP3327637B2 (en) * | 1993-07-14 | 2002-09-24 | 核燃料サイクル開発機構 | Functionally graded composite material of copper and carbon and method for producing the same |
AU686648B2 (en) * | 1993-09-03 | 1998-02-12 | Minnesota Mining And Manufacturing Company | Fluorine cell |
WO2019065258A1 (en) | 2017-09-27 | 2019-04-04 | 積水化学工業株式会社 | Carbon dioxide reduction device, and porous electrode |
CN109267098B (en) * | 2018-09-27 | 2019-10-18 | 四川大学 | Fluorine anode processed and preparation method thereof |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2334638A (en) * | 1940-10-05 | 1943-11-16 | Fort Orange Paper Company | Bottle carrier |
GB1277620A (en) * | 1969-01-31 | 1972-06-14 | Conradty Fa C | Electrodes for electric arc furnaces |
GB2054650A (en) * | 1979-08-02 | 1981-02-18 | Watanabe N | Darbon anode used in electrolytic method of producing fluorine from a potassium fluoride and hydrogen fluoride mixed salt system |
Family Cites Families (14)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2534638A (en) * | 1947-12-17 | 1950-12-19 | Harshaw Chem Corp | Electrolytic production of fluorine |
GB957168A (en) * | 1959-10-02 | 1964-05-06 | Ici Ltd | Improvements in or relating to a process for the electrolytic production of fluorineand apparatus therefor |
US3342910A (en) * | 1963-11-05 | 1967-09-19 | Japan Atomic Energy Res Inst | Process for preparing nuclear fuel elements of dispersed-in-graphite type |
FR1474297A (en) * | 1965-03-26 | 1967-03-24 | Clevite Corp | electrode for fuel cells |
GB1137743A (en) * | 1965-03-26 | 1968-12-27 | Clevite Corp | Fuel cell electrode |
US4011374A (en) * | 1975-12-02 | 1977-03-08 | The United States Of America As Represented By The United States Energy Research And Development Administration | Porous carbonaceous electrode structure and method for secondary electrochemical cell |
US4048715A (en) * | 1976-01-27 | 1977-09-20 | The United States Of America As Represented By The United States Energy Research And Development Administration | Method of preparing porous, active material for use in electrodes of secondary electrochemical cells |
US4282074A (en) * | 1980-07-07 | 1981-08-04 | Ppg Industries, Inc. | Electrolytic process utilizing a transition metal-graphite intercalation compound cathode |
JPS57200585A (en) * | 1981-06-02 | 1982-12-08 | Nikkei Giken:Kk | Carbonaceous electrode plate for manufacture of fluorine by electrolysis |
JPS5928581A (en) * | 1982-08-05 | 1984-02-15 | Asahi Glass Co Ltd | Material for gas diffusion electrode |
JPS60221591A (en) * | 1984-04-17 | 1985-11-06 | Central Glass Co Ltd | Manufacture of fluorine |
EP0163597A1 (en) * | 1984-04-27 | 1985-12-04 | Schweizerische Aluminium Ag | Process for diminution of the tendency towards oxidation at increased temperatures of carbon powders or of shaped carbon articles fabricated by using the afore-mentioned carbon powder |
US4568442A (en) * | 1985-02-01 | 1986-02-04 | The Dow Chemical Company | Gas diffusion composite electrode having polymeric binder coated carbon layer |
DE3538294A1 (en) * | 1985-10-29 | 1987-04-30 | Alusuisse | Method for reducing the oxidation tendency existing at temperatures above 800 DEG C of anodes prepared from carbon powder for the production of aluminium by molten-salt electrolysis |
-
1986
- 1986-08-01 GB GB8618909A patent/GB2193225B/en not_active Expired - Lifetime
-
1987
- 1987-06-23 DE DE8787305563T patent/DE3766564D1/en not_active Expired - Lifetime
- 1987-06-23 EP EP87305563A patent/EP0255225B1/en not_active Expired - Lifetime
- 1987-06-29 CA CA000540822A patent/CA1315240C/en not_active Expired - Fee Related
- 1987-07-15 AU AU75671/87A patent/AU597690B2/en not_active Ceased
- 1987-07-20 ZA ZA875309A patent/ZA875309B/en unknown
- 1987-07-31 JP JP62192511A patent/JPS6338593A/en active Pending
-
1988
- 1988-11-02 US US07/267,616 patent/US4915809A/en not_active Expired - Fee Related
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2334638A (en) * | 1940-10-05 | 1943-11-16 | Fort Orange Paper Company | Bottle carrier |
GB1277620A (en) * | 1969-01-31 | 1972-06-14 | Conradty Fa C | Electrodes for electric arc furnaces |
GB2054650A (en) * | 1979-08-02 | 1981-02-18 | Watanabe N | Darbon anode used in electrolytic method of producing fluorine from a potassium fluoride and hydrogen fluoride mixed salt system |
Also Published As
Publication number | Publication date |
---|---|
EP0255225A2 (en) | 1988-02-03 |
EP0255225A3 (en) | 1988-12-21 |
AU7567187A (en) | 1988-02-18 |
JPS6338593A (en) | 1988-02-19 |
GB2193225A (en) | 1988-02-03 |
DE3766564D1 (en) | 1991-01-17 |
GB8618909D0 (en) | 1986-09-10 |
GB2193225B (en) | 1990-09-19 |
EP0255225B1 (en) | 1990-12-05 |
CA1315240C (en) | 1993-03-30 |
US4915809A (en) | 1990-04-10 |
ZA875309B (en) | 1988-01-26 |
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